Methyl iodide → Methyl 3-methyl-4-oxo-3,4-dihydroimidazo[5,1-d][1,2,3,5]tetrazine-8-carbimidothioate hydroiodide

HRID 570940

反応式

HRID 570940 の反応式
[CH3:1][N:2]1[C:7](=[O:8])[N:6]2[CH:9]=[N:10][C:11]([C:12](=[S:14])[NH2:13])=[C:5]2[N:4]=[N:3]1.[CH3:15][I:16]>C(#N)C>[IH:16].[CH3:1][N:2]1[C:7](=[O:8])[N:6]2[CH:9]=[N:10][C:11]([C:12]([S:14][CH3:15])=[NH:13])=[C:5]2[N:4]=[N:3]1

参加物

4

反応物 2

HCID 6328Methyl iodideHCID 33528803-Methyl-4-oxo-3,4-dihydroimidazo[5,1-d][1,2,3,5]tetrazine-8-carbothioamide

生成物 1

HCID 66831606Methyl 3-methyl-4-oxo-3,4-dihydroimidazo[5,1-d][1,2,3,5]tetrazine-8-carbimidothioate hydroiodide収率 88%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A solution of 3-methyl-4-oxo-3,4-dihydroimidazo[5,1-d][1,2,3,5]tetrazine-8-carbothioamide (2.75 g, 13.1 mmol) and methyl iodide (8.2 mL, 131 mmol) in acetonitrile (900 mL) was stirred at room temperature for 3 days. The mixture was concentrated under vacuum and the solid was suspended in diethyl ether. The precipitate was filtered and washed with diethyl ether to give the pure title compound as an orange solid (4.03 g, 88% yield). δH (DMSO-d6): 11.6 (1H, bs), 9.18 (1H, s) 3.94 (3H, s), 2.82 (3H, s).

後処理

  1. concentrationThe mixture was concentrated under vacuum
  2. filtrationThe precipitate was filtered
  3. washwashed with diethyl ether

出典と根拠

ORDレコード
ord-f5e14e63d54e413c89dae841aa3c9064
出典データセット
uspto-grants-2015_05
特許番号
US09024018B2

関連ノート

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